切向流过滤膜结构与功能
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0 - 45 psi High Flux rates because of open pore structure and permeability of the membrane 开孔结构和膜的通透性决定了高流速
Pore Rating 开孔率
Based on retention of non-deformable particles 决定于不可变形颗粒的截留率
GVWP PVDF 0.22um B.diminuta
Bpt.
HVLP PVDF 0.45um S. marcesens
Bpt.
7
膜孔径选择与产物损失
• 截流率导致的产物损失受以下操作参数影响 – 体积浓缩因子 – 透析体积
• 对于在回流液中的产物损失计算 – % Product Loss to filtrate = 100 * {1 - e[(R - 1)*(ln VCF + N)]} – 3~5倍的余量
16
LN (VCF) + N
8
Membrane Capabilities 膜的功能
Concentration浓缩 –Removal of solvent and smaller solutes 除去溶剂和小分子溶 质 –Retentate is kept 截留率不变
Membrane is selected to retain wanted solute
and the solute 液体和溶质的性质 z Concentrations - initial
and final浓度-初始和最后 z Stability / solubility 稳定性/可溶性 z Effective pore size有效孔径 z Processing sensitivity 过程的敏感性 z Potential hazards 潜在的风险
Feed
Membrane is
selected to pass
unwanted solute
Permeate
while retaining
Filtrate
wanted solute(s)膜被选择透过不要的溶液而截留想要
的溶液
–Also known as "Constant Volume Washing" /
10
Defining the Separation Objective 明确分离的目标
z What is the product solution/suspension to be filtered? z 待过滤的产品溶液/悬浮液是什么?
Îname, composition, properties, stability... Î名字.组成,性质,稳定性 z What must be removed from the product during filtration? z 过滤中什么必须被除去? Îsolvent, other solutes, insolubles, and their characteristics Î溶剂.其他溶液,不溶物和他们的性质 z What are the concentrations of product, solvent, impurities?产品,溶剂,杂质的浓度是多少? z At what temperature should filtration be conducted? z 在多少温度下操作?
Membrane Structure: UF Cross-sectional SEM's 膜结构
PES Membranes 聚砜膜
Conventional PES membranes with finger voids
手指状的传统聚砜膜
Void Free Biomax PES membranes 无缺陷的聚砜膜Biomax
膜的结构和功能
切向流（TFF）过滤高级培训课程
Regenerated Cellulose Composite 30 kD Membrane at 2014x
摘要
z 膜的结构和材质 − 微孔过滤 (MF) − 超滤 (UF) − 反渗透/纳滤 (RO/NF)
z 膜的关键特性 z 分离工艺膜的选择
1
膜的材质
"Buffer Exchange“ – 比如”等体积冲洗””缓冲溶液的置换”
Retentate
Selecting a Membrane for a Separation 如何为分离工艺选择合适的膜?
z Objective of the separation分离的目的 z Characteristics of the fluid
– Adsorption吸附 –Particles are adsorbed into the membrane structure –颗粒被吸附在膜上
Porosity开孔率
– Defined by % of membrane made up by the pores定义膜上开孔的比率 –The higher the porosity the higher the permeability –高开孔率高通透率
PS 30,000 Albumin >98%
Cytochrome C >50%
Gamma Globulin>99% PS 100,000 Gamma Globulin>99%Albumin >20%
RC 300,000 T500 Dextran >70% T70 Dextran >60%
PVDF 300,000 T500 Dextran >60% T70 Dextran >60%
紧密的膜孔结构可在高压下也可获得膜的截留率
Pore Rating 孔径
Based on retention of Globular protein markers for nominal
pore size ratings
相对孔径基于球状蛋白截留率的标定
Single solute testing most common
Protein Mixed Marker Dextran
Test Test
Proteins Dextrans
2 - 3 15 - 20
NO
YBiblioteka BaiduS
NO
YES
YES
NO
YES
NO
YES
NO
NO
YES
NO
YES
Typical Membrane Retention Characteristics 典型的膜截留特征
膜被选择透过想要的溶质
Feed
Retentate
Permeate Filtrate
9
Membrane Capabilities 膜的功能
Diafiltration透析
–Removal of low MW solute 除去小分子溶质
–Retentate is kept 截留不变
Wash +
微孔过滤膜
聚醚砜Polyethersulfone 再生纤维素Regenerated Cellulose 聚偏二氟乙烯PVDF-polyvinylidene fluoride 聚碳酸酯Polycarbonate 尼龙Nylon
超滤膜
聚醚砜Polyethersulfone 再生纤维素Regenerated Cellulose 聚偏二氟乙烯PVDF -polyvinylidene fluoride
复合再生纤维素 Ultracel
降低成本---产物是最重要的因素!
4
Characteristics of UF Membranes 超滤膜的材料特性
Property 膜材质 分子量截留 相对流速 相对截留
蛋白吸附
pH 范围
Biomax™ membranes
聚醚砜 5 kD to 1000 kD
快速
Product Loss to the Filtrate [%]
孔径选择与产物损失 产物在回流液
Product Loss [%] = 100 * {1 - e^[(R - 1)*(ln VCF + N)]}
50
R = 0.8
40
R = 0.9
30
20
R = 0.99
10
R = 0.999
0
0
4
8
12
Diffusion (Testing only detects gross defects)气体扩散
DRYING
孔径定义--葡聚糖截留曲线
6
Mixed Dextran Test vs. Single Protein Marker Test 葡聚糖VS.蛋白标定测试
Test Characteristic
膜被选择截留想要的溶 质
Feed
Retentate
Permeate Filtrate
Membrane Capabilities 膜的功能
Clarification澄清 –Removal of larger solutes – 除去大溶质 –Filtrate is kept – 滤出液不变
Membrane is selected to pass the wanted solute
Ultracel™ PLC membranes
复合再生纤维素
5kD to 1000 kD 1-3kD 非复合
中等
推荐使用30-50% 推荐使用30-50%
分子量截留
分子量截留
低吸附
极低
1 - 14
2 - 13
Microfiltration Membranes 微孔膜参数
Operating Pressure 操作压力
5
Ultrafiltration Membranes 超滤膜参数
Operating Pressure 操作压力
0 - 100 psi (0-6.9 bar)
Tighter pore structure requires higher pressures to overcome
the resistance of the membrane
Type of marker Number of markers Permits membrane QC within a retention band Computerized analysis Retention can vary due to adsorption Retention can vary due to marker shape Retention can vary due to marker charge Control of polarization variability by tangential flow Common set of solutes for different membranes
Filter Code PTGC
PLGC PTTK
PTHK PLMK PKMK
Material NMWL Retention
Passage
Markers
Markers
PS 10,000 Cytochrome C >90% Vitamin B12 > 70%
Albumin >98% RC 10,000 Cytochrome C >95% Vitamin B12 > 70%
膜的材质
– 物理性质
–可压性 –弹性 –韧性
– 化学性质
–pH –溶剂 –化学兼容性
– 热敏性质
–温度
2
Membrane Functionality 膜的功能
Capture mechanisms 捕获机理
– Size Exclusion大小排除 –Surface capture / Entrapment –表面捕获/内部捕获
Structure 结构
Open Cell Structure开放的结构 Track Etched or Cast Membrane蚀刻或铸造膜 Symmetric or asymmetric 相对或绝对
Integrity Testing完整性测试
Bubble point and or Diffusion tests泡点或气体扩散 Correlated to destructive tests关联到破坏性测试
THICKNESS CONTROL
Asymmetric不对称 Finger voids or void-free 手指状或无缺陷 Non-composite or composite非复合或复合
MEMBRANE CASTING HYDROPHILISATION
Integrity Testing完整性测试
通常是单一溶液测试
Mixed solute testing is more realistic but newer
混合溶液测试更现实,但是较新
Structure 结构
MIXING
ENVIRONMENTALY CONTROLLED CHAMBER
Cast Membrane铸造膜 Thin skin薄皮
3
Membrane Structure: UF Cross-sectional SEM's 膜结构
Regenerated Cellulose 再生纤维素
Conventional Regenerated Cellulose传统再生纤维素
Composite Regenerated Cellulose Ultracel
Pore Rating 开孔率
Based on retention of non-deformable particles 决定于不可变形颗粒的截留率
GVWP PVDF 0.22um B.diminuta
Bpt.
HVLP PVDF 0.45um S. marcesens
Bpt.
7
膜孔径选择与产物损失
• 截流率导致的产物损失受以下操作参数影响 – 体积浓缩因子 – 透析体积
• 对于在回流液中的产物损失计算 – % Product Loss to filtrate = 100 * {1 - e[(R - 1)*(ln VCF + N)]} – 3~5倍的余量
16
LN (VCF) + N
8
Membrane Capabilities 膜的功能
Concentration浓缩 –Removal of solvent and smaller solutes 除去溶剂和小分子溶 质 –Retentate is kept 截留率不变
Membrane is selected to retain wanted solute
and the solute 液体和溶质的性质 z Concentrations - initial
and final浓度-初始和最后 z Stability / solubility 稳定性/可溶性 z Effective pore size有效孔径 z Processing sensitivity 过程的敏感性 z Potential hazards 潜在的风险
Feed
Membrane is
selected to pass
unwanted solute
Permeate
while retaining
Filtrate
wanted solute(s)膜被选择透过不要的溶液而截留想要
的溶液
–Also known as "Constant Volume Washing" /
10
Defining the Separation Objective 明确分离的目标
z What is the product solution/suspension to be filtered? z 待过滤的产品溶液/悬浮液是什么?
Îname, composition, properties, stability... Î名字.组成,性质,稳定性 z What must be removed from the product during filtration? z 过滤中什么必须被除去? Îsolvent, other solutes, insolubles, and their characteristics Î溶剂.其他溶液,不溶物和他们的性质 z What are the concentrations of product, solvent, impurities?产品,溶剂,杂质的浓度是多少? z At what temperature should filtration be conducted? z 在多少温度下操作?
Membrane Structure: UF Cross-sectional SEM's 膜结构
PES Membranes 聚砜膜
Conventional PES membranes with finger voids
手指状的传统聚砜膜
Void Free Biomax PES membranes 无缺陷的聚砜膜Biomax
膜的结构和功能
切向流（TFF）过滤高级培训课程
Regenerated Cellulose Composite 30 kD Membrane at 2014x
摘要
z 膜的结构和材质 − 微孔过滤 (MF) − 超滤 (UF) − 反渗透/纳滤 (RO/NF)
z 膜的关键特性 z 分离工艺膜的选择
1
膜的材质
"Buffer Exchange“ – 比如”等体积冲洗””缓冲溶液的置换”
Retentate
Selecting a Membrane for a Separation 如何为分离工艺选择合适的膜?
z Objective of the separation分离的目的 z Characteristics of the fluid
– Adsorption吸附 –Particles are adsorbed into the membrane structure –颗粒被吸附在膜上
Porosity开孔率
– Defined by % of membrane made up by the pores定义膜上开孔的比率 –The higher the porosity the higher the permeability –高开孔率高通透率
PS 30,000 Albumin >98%
Cytochrome C >50%
Gamma Globulin>99% PS 100,000 Gamma Globulin>99%Albumin >20%
RC 300,000 T500 Dextran >70% T70 Dextran >60%
PVDF 300,000 T500 Dextran >60% T70 Dextran >60%
紧密的膜孔结构可在高压下也可获得膜的截留率
Pore Rating 孔径
Based on retention of Globular protein markers for nominal
pore size ratings
相对孔径基于球状蛋白截留率的标定
Single solute testing most common
Protein Mixed Marker Dextran
Test Test
Proteins Dextrans
2 - 3 15 - 20
NO
YBiblioteka BaiduS
NO
YES
YES
NO
YES
NO
YES
NO
NO
YES
NO
YES
Typical Membrane Retention Characteristics 典型的膜截留特征
膜被选择透过想要的溶质
Feed
Retentate
Permeate Filtrate
9
Membrane Capabilities 膜的功能
Diafiltration透析
–Removal of low MW solute 除去小分子溶质
–Retentate is kept 截留不变
Wash +
微孔过滤膜
聚醚砜Polyethersulfone 再生纤维素Regenerated Cellulose 聚偏二氟乙烯PVDF-polyvinylidene fluoride 聚碳酸酯Polycarbonate 尼龙Nylon
超滤膜
聚醚砜Polyethersulfone 再生纤维素Regenerated Cellulose 聚偏二氟乙烯PVDF -polyvinylidene fluoride
复合再生纤维素 Ultracel
降低成本---产物是最重要的因素!
4
Characteristics of UF Membranes 超滤膜的材料特性
Property 膜材质 分子量截留 相对流速 相对截留
蛋白吸附
pH 范围
Biomax™ membranes
聚醚砜 5 kD to 1000 kD
快速
Product Loss to the Filtrate [%]
孔径选择与产物损失 产物在回流液
Product Loss [%] = 100 * {1 - e^[(R - 1)*(ln VCF + N)]}
50
R = 0.8
40
R = 0.9
30
20
R = 0.99
10
R = 0.999
0
0
4
8
12
Diffusion (Testing only detects gross defects)气体扩散
DRYING
孔径定义--葡聚糖截留曲线
6
Mixed Dextran Test vs. Single Protein Marker Test 葡聚糖VS.蛋白标定测试
Test Characteristic
膜被选择截留想要的溶 质
Feed
Retentate
Permeate Filtrate
Membrane Capabilities 膜的功能
Clarification澄清 –Removal of larger solutes – 除去大溶质 –Filtrate is kept – 滤出液不变
Membrane is selected to pass the wanted solute
Ultracel™ PLC membranes
复合再生纤维素
5kD to 1000 kD 1-3kD 非复合
中等
推荐使用30-50% 推荐使用30-50%
分子量截留
分子量截留
低吸附
极低
1 - 14
2 - 13
Microfiltration Membranes 微孔膜参数
Operating Pressure 操作压力
5
Ultrafiltration Membranes 超滤膜参数
Operating Pressure 操作压力
0 - 100 psi (0-6.9 bar)
Tighter pore structure requires higher pressures to overcome
the resistance of the membrane
Type of marker Number of markers Permits membrane QC within a retention band Computerized analysis Retention can vary due to adsorption Retention can vary due to marker shape Retention can vary due to marker charge Control of polarization variability by tangential flow Common set of solutes for different membranes
Filter Code PTGC
PLGC PTTK
PTHK PLMK PKMK
Material NMWL Retention
Passage
Markers
Markers
PS 10,000 Cytochrome C >90% Vitamin B12 > 70%
Albumin >98% RC 10,000 Cytochrome C >95% Vitamin B12 > 70%
膜的材质
– 物理性质
–可压性 –弹性 –韧性
– 化学性质
–pH –溶剂 –化学兼容性
– 热敏性质
–温度
2
Membrane Functionality 膜的功能
Capture mechanisms 捕获机理
– Size Exclusion大小排除 –Surface capture / Entrapment –表面捕获/内部捕获
Structure 结构
Open Cell Structure开放的结构 Track Etched or Cast Membrane蚀刻或铸造膜 Symmetric or asymmetric 相对或绝对
Integrity Testing完整性测试
Bubble point and or Diffusion tests泡点或气体扩散 Correlated to destructive tests关联到破坏性测试
THICKNESS CONTROL
Asymmetric不对称 Finger voids or void-free 手指状或无缺陷 Non-composite or composite非复合或复合
MEMBRANE CASTING HYDROPHILISATION
Integrity Testing完整性测试
通常是单一溶液测试
Mixed solute testing is more realistic but newer
混合溶液测试更现实,但是较新
Structure 结构
MIXING
ENVIRONMENTALY CONTROLLED CHAMBER
Cast Membrane铸造膜 Thin skin薄皮
3
Membrane Structure: UF Cross-sectional SEM's 膜结构
Regenerated Cellulose 再生纤维素
Conventional Regenerated Cellulose传统再生纤维素
Composite Regenerated Cellulose Ultracel